透射电子显微镜侧插式CCD相机数字图片放大倍数的解析

针对数字化透射电子显微镜与传统透射电子显微镜在观察记录系统上存在的差异,通过比较分析数字化透射电子显微镜侧插式电荷耦合器件(CCD)相机采集的图像、操作界面View视窗观察到的图像与电镜示数放大倍数之间的差异,详细地分析了数字化透射电子显微镜侧插式CCD相机采集的数字图片的放大倍数发生变化的原因.可以帮助应用电镜的广大教师及科研工作者更加快速、直观地掌握数字图片确切的放大倍数,更有利于结果的分析.     

Off-axis STEM or TEM holography combined with four-dimensional diffraction imaging.

Ultrahigh-resolution imaging may be achieved using modifications of the off-axis holography scheme in a scanning transmission electron microscopy (STEM) instrument equipped with one or more electrostatic biprisms in the illuminating system. The resolution is governed by the diameter of a reference beam, reduced by channeling through a line of atoms in an atomic-focuser crystal. Alternatively, the off-axis holography may be combined with the Rodenburg method in which a four-dimensional data set is obtained by recording a nanodiffraction pattern from each point of the specimen as the incident beams are scanned. An ultrahigh-resolution image is derived by computer processing to give a particular two-dimensional section of this data set. The large amount of data recording and data processing involved with this method may be avoided if the two-dimensional section is derived by recording the hologram while the four beams produced by two perpendicular biprisms are scanned in opposing directions across the specimen by varying the voltages on the biprisms. An equivalent scheme for conventional TEM is also possible. In each case, the complex transmission function of the specimen may be derived and resolutions of about 0.05 nm may be expected.     

A Novel Method of Analytical Transmission Electron Microscopy for Measuring Highly Accurately Segregation to Special Grain Boundaries or Planar Interfaces

A new technique of analytical transmission electron microscopy has been developed for determining accurately the amount of solute atoms incorporated into well-defined planar defects in solids, such as stacking faults, special grain boundaries or interfaces. The method is based on recording series of analytical spectra taken with different electron beam diameters on the same position centred above a defect that is oriented nearly edge-on. The matrix/solute ratio is then plotted as a function of the electron beam radius, linear regression is performed and the segregation level is determined from the slope of the best fit. This method can be applied to energy-dispersive X-ray (EDX) or electron energy-loss spectroscopy (EELS) in a transmission electron microscope. It necessitates a nano-probe mode but no scan unit. Reliability and accuracy have been tested numerically. Simulations suggest an accuracy in the determination of the Gibbsian solute excess at a special grain boundary down to ±0.1 atoms nm⁻² under typical experimental conditions, with a maximum error about twice as large.     

Characterization of Fe/Cr multilayers by analytical transmission electron microscopy

Different techniques of analytical TEM were used to investigate Fe/Cr multilayers. These multilayers show a dependence of their electrical resistance as a function of the magnetic field. This effect called giant magnetoresistance can be utilized for example in magnetic recording heads. Typical dimensions of the single layer thickness are in the nanometer region. Therefore the microstructure of this material has been investigated by transmission electron microscopy (TEM). To get additional analytical information energy dispersive X-ray spectroscopy (EDXS) and electron energy loss spectroscopy (EELS) can be used. Received: 15 July 1997 / Revised: 5 February 1998 / Accepted: 6 February 1998     

Multiple scattering Xα calculations on the Σ and it electron shape resonances in chloroethylenes and fluoroethylenes

The continuum OS MS Xα method is used to interpret the multiple resonances observed in the electron transmission spectra of tetrachloroethylene and 1,1-dichloroethylene. Good agreement with experiment is found for these molecules and for their fluorine analogues which exhibit one shape resonance. Dissociative electron attachment studies on the halogenoethylenes are interpreted in detail.     

Nucleation and growth of silver nanoparticles monitored by titration microcalorimetry

The nucleation and the growth of silver nanoparticles were studied by spectrophotometry and transmission electron microscopy, with simultaneous recording of the concomitant enthalpy changes. Silver nanoparticles were stabilized by sodium citrate and reduction was brought about by the addition of hydroquinone in aqueous medium. It was established that nucleation is an exothermic process and heat effects are basically determined by the ratio of silver ions to hydroquinone. The process of nanoparticle formation was divided to three phases: the nucleation phase is exothermic, the growth phase is endothermic and further addition of the reducing agent results in the aggregation of silver nanoparticles, which produces a second exothermic heat effect.     

Tutorial on off-axis electron holography.

Through recent years, off-axis electron holography has helped us to understand and to overcome some experimental restrictions in transmission electron microscopy. With development of powerful electron microscopes, slow-scan CCD cameras, and computers, holography is not an academic technique anymore used by specialized laboratories. Holography has proven its wide range of applications in solving real-world problems in materials science and biology. At medium resolution, that is, on nanometer scale, holography allows access to large area phase contrast produced by magnetic fields and electric potentials. In the high-resolution domain, holography unveils its power by unscrambling amplitude and phase of the electron wave, resulting in an improved lateral resolution up to the information limit. Holography is a thoroughly quantitative method, and, in combination with the perfect zero-loss filtering inherent to this method, the interpretation of the reconstructed data is strongly simplified. After outlining the basics of holography, in this tutorial we focus on development of a step-by-step procedure for recording and reconstruction of holograms. At the end, some recent applications are discussed.     

EELS nanoanalysis for investigating both chemical composition and bonding of interlayers in composites

The paper is concerned with the application of analytical transmission electron microscopy (TEM) to characterize both chemical composition and bond state of the elements detected in interlayers in C- and SiC-fibre reinforced composites. The chemical bond state of nanometre-sized regions is characterized by means of electron energy loss spectroscopy (EELS), where respective information is gained by analysing energy loss near edge structures (ELNES). In this context results of Si-L₂₃ ELNES investigations are presented concerning the chemical bonding of silicon with carbon, nitrogen and oxygen. The specific bond state of silicon is revealed by recording series of EEL spectra at high energy resolution across the fibre/ matrix interlayers of interest. Moreover, the element distribution is imaged by energy-filtered TEM.Dedicated to Professor Dr. rer.nat. Dr. h.c. Hubertus Nickel on the occasion of his 65th birthday     

树脂包埋在透射电子显微镜测试中的应用

在环氧树脂包埋样品的过程中,部分样品易漂浮于树脂中而不易定位,因而影响了技术人员超薄切片的效率及样品在透射电子显微镜下的观察效果.对易漂浮于环氧树脂中的样品进行多次包埋定位,再通过修块、切片等步骤制备透射电子显微镜截面样品,特别适用于快速高效地制备纳米线、棒等截面样品.多次包埋方法操作简单、实用性强,经超薄切片后制备出的样品截面更清晰、更完整.     

The Crystal Structure of Orthocetamol Solved by 3D Electron Diffraction

Orthocetamol is a regioisomer of the well‐known pain medication paracetamol and a promising analgesic and an anti‐arthritic medicament itself. However, orthocetamol cannot be grown as single crystals suitable for X‐ray diffraction, so its crystal structure has remained a mystery for more than a century. Here, we report the ab‐initio structure determination of orthocetamol obtained by 3D electron diffraction, combining a low‐dose acquisition method and a dedicated single‐electron detector for recording the diffracted intensities. The structure is monoclinic, with a pseudo‐tetragonal cell that favors multiple twinning on a scale of a few tens of nanometers. The successful application of 3D electron diffraction to orthocetamol introduces a new gold standard of total structure solution in all cases where X‐ray diffraction and electron‐microscope imaging methods fail.     

Electron holography with a Cs-corrected transmission electron microscope.

Cs correctors have revolutionized transmission electron microscopy (TEM) in that they substantially improve point resolution and information limit. The object information is found sharply localized within 0.1 nm, and the intensity image can therefore be interpreted reliably on an atomic scale. However, for a conventional intensity image, the object exit wave can still not be detected completely in that the phase, and hence indispensable object information is missing. Therefore, for example, atomic electric-field distributions or magnetic domain structures cannot be accessed. Off-axis electron holography offers unique possibilities to recover completely the aberration-corrected object wave with uncorrected microscopes and hence we would not need a Cs-corrected microscope for improved lateral resolution. However, the performance of holography is affected by aberrations of the recording TEM in that the signal/noise properties ("phase detection limit") of the reconstructed wave are degraded. Therefore, we have realized off-axis electron holography with a Cs-corrected TEM. The phase detection limit improves by a factor of four. A further advantage is the possibility of fine-tuning the residual aberrations by a posteriori correction. Therefore, a combination of both methods, that is, Cs correction and off-axis electron holography, opens new perspectives for complete TEM analysis on an atomic scale.     

Studies of orientation and structure of crazed matter in polystyrene. II. Electron diffraction measurements

The technique of selected area electron diffraction in the transmission electron microscope is used to examine the degree of orientation of crazed matter. The theories of electron and x-ray diffraction are compared and it is shown experimentally, by comparison with published x-ray results, that it is possible to obtain electron diffraction patterns from uncrazed polystyrene that are reasonably free of both radiation damage and multiple scattering problems. Electron diffraction patterns from crazes show a considerable degree of orientation but otherwise are very similar to those from uncrazed material, showing that crazes have no structure different from that of bulk material. Diffraction patterns are also obtained from thin films drawn to draw ratios of 4.5 and 6 at 90°C. These agree well with published x-ray results from oriented polystyrene but show less anisotropy than the craze diffraction patterns.     

具多重氢键寡聚芳酰胺的合成及自组装

含六重氢键寡聚芳酰胺双分子链在没有相应互补链的情况下, 其中一条链发生自组装. 通过紫外-可见(UV-Vis)光谱、动态光散射(DLS)、扫描电镜(SEM)和透射电镜(TEM)等实验手段, 对其自组装行为进行了研究. 实验结果表明, 在1,2-二氯乙烷中随温度升高在紫外区吸收发生蓝移, 说明酰胺自组装体部分解聚. 该分子链在不同极性的溶剂中都能发生自组装, 并随极性不同表现为不同的形貌. 如在甲苯中呈网状结构, 在极性相对较弱的二氯甲烷和环己烷的混合溶剂中为不规则的蜂窝状结构, 而在三氯甲烷和甲醇组成的极性混合溶剂中则组装成稳定的实心微球, 其直径随着浓度升高而增大, 通过在乙腈中的降温过程, 观察到组装体形貌由管状纤维向实心球的转变.     

Mapping the chemistry in nanostructured materials by energy-filtering transmission electron microscopy (EFTEM)

Energy-filtered transmission electron microscopy (EFTEM) can be used to acquire elemental distribution maps at high lateral resolution within short acquisition times, which makes it quite efficient for a detailed characterization of nanostructures, as illustrated with examples concerning a nanostructured substituted La-based cermet compound and a nanoscale multilayer. In the first example, we show how phases in a rapidly cooled substituted LaNi5 can be visualized by recording jump ratio images. Secondly, EFTEM was capable of imaging individual nanoscale layers in a magnetic multilayer consisting of 2 nm terbium and 3 nm iron.     

Size-dependent morphology of dealloyed bimetallic catalysts: linking the nano to the macro scale

Chemical dealloying of Pt binary alloy precursors has emerged as a novel and important preparation process for highly active fuel cell catalysts. Dealloying is a selective (electro)chemical leaching of a less noble metal M from a M rich Pt alloy precursor material and has been a familiar subject of macroscale corrosion technology for decades. The atomic processes occurring during the dealloying of nanoscale materials, however, are virtually unexplored and hence poorly understood. Here, we have investigated how the morphology and intraparticle composition depend on the particle size of dealloyed Pt-Co and Pt-Cu alloy nanoparticle precursor catalysts. To examine the size-morphology-composition relation, we used a combination of high-resolutionscanning transmission electron microscopy (STEM), transmission electron microscopy (TEM), electron energy loss (EEL) spectroscopy, energy-dispersive X-ray spectroscopy (EDS), and surface-sensitive cycling voltammetry. Our results indicate the existence of three distinctly different size-dependent morphology regimes in dealloyed Pt-Co and Pt-Cu particle ensembles: (i) The arrangement of Pt shell surrounding a single alloy core ("single core-shell nanoparticles") is exclusively formed by dealloying of particles below a characteristic diameter d(multiple cores) of 10-15 nm. (ii) Above d(multiple cores), nonporous bimetallic core-shell particles dominate and show structures with irregular shaped multiple Co/Cu rich cores ("multiple cores-shell nanoparticles"). (iii) Above the second characteristic diameter d(pores) of about 30 nm, the dealloyed Pt-Co and Pt-Cu particles start to show surface pits and nanoscale pores next to multiple Co/Cu rich cores. This structure prevails up to macroscopic bulklike dealloyed particles with diameter of more than 100 nm. The size-morphology-composition relationships link the nano to the macro scale and provide an insight into the existing material gap of dealloyed nanoparticles and highly porous bulklike bimetallic particles in corrosion science.     

A new method of recording diffraction patterns in gas-phase electron diffraction

A new design of the recording unit of an electron diffractometer for gas-phase electron diffraction has been suggested, in which a fixed luminescent screen is used instead of photo plates. The diffraction pattern of a compound displayed on the screen is input to a reading device with contact photographic recording and is transmitted to a computer as digital two-dimensional intensity maps.     

Formation of ZnSe and CdS quantum dots via laser ablation in liquids

Formation of nanoparticles of both ZnSe and CdS under ablation of corresponding bulk semiconductors in liquid environment (diethyleneglycol, ethanol, etc.) using radiation of a Cu vapor laser is reported. X-ray diffraction (XRD), resonance Raman scattering (RRS), and transmission electron microscopy (TEM) confirm that the nanoparticles are crystalline and have average size of ca 10–20 nm. RRS of nanoparticles are characterized by several peaks multiple to frequency of corresponding phonon (LO replicas).     

Low-energy-loss EFTEM imaging of thick particles and aggregates

Electron spectroscopy imaging is a powerful tool for the elucidation of colloidal particle morphology and microchemistry, but it normally requires the use of very thin samples, typically less than 50 nm, to avoid the effects of multiple scattering. This work shows that many aspects of the internal morphology of thick particles and aggregates and the chemical component distribution are revealed using low-energy-loss electron imaging in the transmission electron microscope, benefiting from multiple scattering as well as small but significant differences in the low-energy-loss spectra of aggregate constituents. Low-loss images reveal morphological details of thick aggregates made out of colloidal polymers (natural rubber and styrene-acrylic latex) and inorganic particles (silica, montmorillonite, and aluminum phosphate) at a spatial resolution close to that achieved in the bright-field images and much better than in the elemental maps, showing the advantages of the simultaneous use of low-loss images and standard thin-cut elemental maps.     

Application of The Xα and PM3 Methods to Chloromethanes: Ionization Potentials and Electron Affinities

The resonance energies for attachment of an electron to the chloromethanes and the ionization potentials of the chloromethanes were studied both by the multiple scattering Xα-SCF method and by the PM3 method. An external positively charged Watson sphere is used to stabilize the resonances in the Xα method. The calculated results provide support for the assignment of the features observed in the electron transmission spectra of the chloromethanes.     

Methods for investigation of holographic photopolymer materials

Results obtained by the authors on the development of holographic methods for investigation of photopolymer materials are presented. The work considers the methods for pulse recording of dynamic transmission gratings and characterization of hologram angular selectivity, the double-beam method of twophoton holographic recording, and heterodyne detection of inhomogeneities in volume holograms.